recognized
`principles on standardization established in the Decision on Principles for the
`This international standard was developed in accordance with internationally
`Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
`
`Ally Designation: D5757-22
`
`‘ud
`INTERNATIONAL
`
`Standard Test Method for
`Determination of Attrition of FCC Catalysts by Air Jets'
`
`This standard is issued under the fixed designation D5757; the number immediately following the designation indicates the year of
`original adoption or, in the case of revision, the year of last revision. A numberin parentheses indicates the year of last reapproval. A
`superscript epsilon (<) indicates an editorial change since the last revision or reapproval.
`
`1. Scope
`1.1 This test method covers the determinationofthe relative
`attrition characteristics of FCC catalysts by means ofair jet
`attrition. Other fine powder catalysts can be analyzed by this
`test method, but the precision of this test method has been
`determined only for FCC catalysts. It is applicable to spheri-
`cally or irregularly shaped particles which range in size
`between 10 and 180 pm, have skeletal densities between 2.4
`and 3.0 g4m° (2400 and 3000 kg/n*) (see IEEE/ASTM SI-
`10) and are insoluble in water. Particles less than 20 um are
`considered fines. (See Terminology D3766.)
`1.2 Units—The valuesstated in SI units are to be regarded
`as standard. No other units of measurementare included in this
`standard.
`
`1.3 This standard does not purport to address all of the
`safety concerns,
`if any, associated with its use. It is the
`responsibility of the user of this standard to establish appro-
`priate safety, health, and environmental practices and deter-
`mine the applicability of regulatory limitations prior to use.
`1.4 This international standard was developed in accor-
`dance with internationally recognized principles on standard-
`ization established in the Decision on Principles for the
`Development of International Standards, Guides and Recom-
`mendations issued by the World Trade Organization Technical
`Barriers to Trade (TBT) Committee.
`
`2. Referenced Documents
`
`2.1 ASTM Standards:?
`D3766 Terminology Relating to Catalysts and Catalysis
`E105 Guide for Probability Sampling of Materials
`E177 Practice for Use of the Terms Precision and Bias in
`ASTM Test Methods
`E456 Terminology Relating to Quality and Statistics
`
`‘This test method is under the jurisdiction of ASTM Committee D32 on
`Catalysts and is the direct responsibility of Subcommittee D32.02 on Physical-
`Mechanical Properties.
`Current edition approved Oct. 1, 2022. Published October 2022. Originally
`approved in 1995. Last previous edition approved in 2017 as D5757 — 11(2017).
`DOI: 10.1520/D5757-22.
`
`? For referenced ASTM standards, visit the ASTM website, www.astm.org, or
`contact ASTM Customer Service at service@astm.org. For Annual Book ofASTM
`Standards volume information, refer to the standard’s Document Summary page on
`the ASTM website.
`
`E691 Practice for Conducting an Interlaboratory Study to
`Determine the Precision of a Test Method
`IEEE/ASTM SI-10 Standard for Use of the International
`System of Units (SI): The Modern Metric System
`
`3. Terminology
`
`3.1 Definitions of Terms Specific to This Standard:
`3.1.1 Air Jet Index (AJI), n—a unitless value numerically
`equal to the percentattrition loss at 5 h.
`
`4. Summary of Test Method
`4.1 A sample of dried powder is humidified and attrited by
`meansof three high velocity jets of humidified air. The fines
`are continuously removedfrom theattrition zone by elutriation
`into a fines collection assembly.
`4.2 The AJI is calculated from the elutriated fines to give a
`relative estimate of the attrition resistance of the powdered
`catalyst as may be observed in commercial use.
`
`5. Significance and Use
`5.1 This test method is intended to provide information
`concerning the ability of a powdered catalyst to resist particle
`size reduction during use in a fluidized environment.
`5.2 This test method is suitable for specification acceptance,
`manufacturing control, and research and development pur-
`poses.
`
`6. Apparatus
`6.1 The air jet attrition system consists of the following:
`6.1.1 Attrition Tube, a stainless steel tube 710 mm long with
`a 35 mm inside diameter.
`
`Note 1—NPS 1% in. pipe, Schedule 40 has the appropriate inside
`diameter.
`
`6.1.2 Three 2mm Long Drilled Sapphire Square Edged
`Nozzles, precision drilled 0.381 + 0.005 mm in diameter. They
`are mounted equidistant from each other, 10 mm from center
`and flush with the top surface in a circular orifice plate 6.4 mm
`thick. The plate is designed to be attached to the bottom of the
`vertical attrition tube within an air delivery manifold.
`6.1.3 Settling Chamber, a 300mm long cylinder with a
`110 mm inside diameter and with conical ends reducing to
`30mm inside diameter. The upper cone is approximately
`
`Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
`
`WRG-1010
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`ily p5757 - 22
`100 mm long and the lower cone is approximately 230 mm
`7.4.3 Mix 45 g of the dried and cooled material thoroughly
`long. The chamber is mounted to the top of the attrition tube.
`with 5 g of demineralized water ensuring that the water is well
`6.1.4 Fines Collection Assembly, made up of a 250 mL
`dispersed and that there are no lumps of material present.
`filtering flask, an extraction thimble connected to the side arms
`7.4.4 Allow the sample to stand over a saturated calcium
`chloride solution in a humidifier for 1 h.
`of the flask, and a 200 by 13 mm diameter metal tubing bentto
`an angle of 125° connectingthe topof the flask to the top of the
`settling chamber.
`
`Note 2—The flask may be eliminated and the thimble connected
`directly to the tubingif the attrition is expected to be low enough to avoid
`clogging the thimble and creating a backpressure in the settling chamber.
`6.1.5 Rubber Couplers and Seals, appropriately sized to
`ensure tight and leak free connections of the system.
`6.2 Air Supply Source, controlled and capable of maintain-
`ing an air flow rate of 10.00 L/min stable to 0.05 L/min at a
`pressure up to 200 kPa. The air mustbe at a relative humidity
`of 30 to 40 % to minimize electrostatic effects.
`
`Note 3—The air may be bubbled through a 0.25 m column of deionized
`water at ambient temperature to obtain the required humidity.
`6.3 Diaphragm-Type Test Meter (Dry Test Meter) or Liquid-
`Sealed Rotating Drum Meter (Wet Test Meter), minimum
`capacity of 30 LAnin and maximum scale subdivision of 0.1 L
`or electronic mass flow controllers may be used.
`6.4 Balance, 400 g capacity open pan with 0.01 g sensitiv-
`ity.
`6.5 Desiccator, with a desiccant grade molecular sieve such
`as 4A.
`
`6.6 Muffle Furnace.
`6.7 Relative Humidity Gage.
`
`7. Sampling
`7.1 Obtain a representative sample of approximately 65 g of
`material from larger composites by riffling or splitting in
`accordance with subsection 5.12 of STP 447A? or some other
`suitable means with the aim of obtaining a sample that
`represents the size distribution of the larger composite. The
`analyst should also consult Guide E105 to help develop a
`sampling plan.
`
`7.2 Gently screen the sample through a No. 80 (180 um)
`ASTM sieve to remove any particles larger than 180 pm.
`7.3 The step in 7.3.1 is followed for all samples except fresh
`FCC catalysts for proper equilibration at 35 % humidity to
`avoid absorption of water during thetest.
`7.3.1 Transfer the presieved sample to a shallow wide dish
`and place in a humidifier over a saturated calcium chloride
`solution for 16 h.
`
`7.4 The steps in 7.4.1 — 7.4.4 are followed for fresh FCC
`catalysts to ensure a proper moisture level that will not change
`during the test.
`7.4.1 Transfer the presieved sample to a shallow dish and
`dry it for 1 h in a muffle furnace preheated to 565 °C.
`7.4.2 Cool the sample to room temperature in a desiccator.
`
`8. Preparation of Apparatus
`8.1 Thoroughly clean any residual material from the appa-
`tratus by tapping it loose and blowing or vacuuming the dust.
`Reassemble the system except for the fines collection assem-
`bly.
`8.2 Turn on the air supply and adjust the relative humidity
`ofthe air exiting the settling chamberto a range of 30 to 40 %.
`8.3 Connectthe inlet of the wet test gas meterto the top of
`the settling chamber and adjust the humidified air flow to 10.00
`+ 0.05 LAnin at standard temperature and pressure (STP)
`(273.15 K and 101.325 kPa). The back pressure should be in
`the range of 130 to 180 kPa;if it is not, check that the air jet
`nozzles are clean and within specifications and that there are no
`leaks in the apparatus connections.
`
`Note 4—The backpressure of 130 to 180 kPa should be determined by
`a gauge or transducer installed relatively near the chamber.
`8.4 Prepare two fines collection assemblies and condition
`the thimbles by installing them on the apparatus in succession
`and passing the humidified air through the apparatus for 30 min
`each.
`
`9. Procedure
`
`9.1 Weigh the first conditioned fines collection assembly to
`the nearest 0.01 g and record its mass.
`9.2 With the air flowing at the prescribed 10.00 L/Anin and
`the fines collection assembly off, charge 50 g of water equili-
`brated sample to the apparatus through the top ofthe settling
`chamber, quickly secure the first fines collection assembly to
`the apparatus andstart the timekeeping.
`9.3 Weigh the second conditioned fines collection assembly
`to the nearest 0.01 g and record its mass.
`9.4 After exactly 1h from the start, replace the first fines
`collection assembly with the second one. Weigh and record the
`massofthe first fines collection assembly.
`9.5 After exactly 5h from the start, remove the fines
`collection assembly, weigh it, and record its mass.
`9.6 Turn off the apparatus and disassemble.
`9.7 Recover the sample from the attrition tube and settling
`chamber and weigh to the nearest 0.01 g.
`9.8 Clean the apparatus.
`
`10. Calculations
`
`10.1 Calculate the percent fines lost in the first hour as
`follows:
`
`fines loss, % = (m, — m,)/m, X 100
`
`(1)
`
`where:
`
`3STP 447A, Manual on Test Sieving Methods, ASTM International, West
`Conshohocken, PA 19428
`
`mM, = massofthe first empty fines collection assembly at the
`start of the test, g,
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`

`

`ily p5757 - 22
`m, = massofthe first fines collection assemblyat 1 h, g, and
`m, = mass of the sample charged to apparatus (nominally
`50 g).
`10.2 Calculate the percentfineslost from attrition at the fifth
`hour as follows:
`
`TABLE 1 Repeatability and Reproducibility
`Test Result-AJl
`95% Repeatability Interval
`95 % Reproducibility Interval
`(consensus mean)
`(within laboratory)
`(between laboratories)
`2.530
`0.226 (8.95 % of mean)
`0.907 (35.9 % of mean)
`4.209
`0.279 (6.64 % of mean)
`1.939 (46.1 % of mean)
`20.353
`1.121 (5.51 % of mean)
`11.370 (55.9 % of mean)
`39.945
`1.414 (3.54 % of mean)
`12.029 (30.1 % of mean)
`
`attrition loss, % = (m, — m,+m,— m',)/m, X 100
`
`(2)
`
`where:
`
`m', = mass of the second empty fines collection assembly, g,
`and
`ms = massofthe secondfines collection assembly at 5 h, g.
`10.3 Calculate the percent sample recovery after the test as
`follows:
`
`recovery, % = (m,+m,+m,— m, — m',)/m, x 100
`
`(3)
`
`where:
`
`m, = mass of the sample recovered from the attrition tube
`and the settling chamber.
`
`11. Report
`11.1 Report the following information:
`11.1.1 The AJI, that is, the percentattrition loss at 5 h.
`11.1.2 The first hour fines loss as percent.
`11.1.3 The recovery as percent.
`
`12. Precision and Bias
`
`separate test materials in four to seven separate laboratories.
`Practice E691, modified for nonuniform data sets, was fol-
`lowed for the data reduction. Analysis details are in the
`research report.
`
`12.2 Precision—Pairs oftest results obtained by a procedure
`similar to that described in the study are expected to differ in
`absolute value by less than 2.772 S, where 2.772 S is the 95 %
`probability interval limit on the difference between two test
`results, and S is the appropriate estimate of standard deviation.
`Definitions and usage are given in Practices E456 and E177,
`respectively. See Table 1.
`
`12.3 Bias—The procedure in this test method for measuring
`attrition has no known bias because the value ofthe attrition
`loss is defined only in terms of this test method.
`
`12.1 Test Program—An interlaboratory study was con-
`ducted in which the named property was measured in four
`
`13. Keywords
`13.1 abrasion;air jet; attrition; fines; powdered catalysts
`
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`
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